#------------------------------------------------------------------------------
#$Date: 2020-03-25 04:51:01 +0200 (Wed, 25 Mar 2020) $
#$Revision: 249690 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/01/7240176.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7240176
loop_
_publ_author_name
'Collings, Ines'
'Saines, Paul James'
'Mikolasek, Mirko'
'Boffa Ballaran, Tiziana'
'Hanfland, Michael'
_publ_section_title
;
 Static disorder in a perovskite mixed-valence metal--organic framework
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00119H
_journal_year                    2020
_chemical_formula_moiety         '(C2 H8 N1)0.75, (Fe C3 O6 H3), (H2 O)0.25'
_chemical_formula_sum            'C4.5 H9.5 Fe N0.75 O6.25'
_chemical_formula_weight         229.98
_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_Hall           '-I 2 2 3'
_space_group_name_H-M_alt        'I m -3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-01-23 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.04747(16)
_cell_length_b                   12.04747(16)
_cell_length_c                   12.04747(16)
_cell_measurement_reflns_used    4144
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.5720
_cell_measurement_theta_min      4.0780
_cell_volume                     1748.59(4)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2014)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2014)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10362
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.227
_diffrn_reflns_theta_min         3.382
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       cube
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         445
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0493P)²+3.9725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                348
_reflns_number_total             445
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00119h2.cif
_cod_data_source_block           DMAFeFe_H2O-4
_cod_original_cell_volume        1748.59(7)
_cod_original_formula_sum        'C4.50 H9.50 Fe N0.75 O6.25'
_cod_database_code               7240176
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.875
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.250000 0.250000 0.250000 0.0218(3) Uani 1 6 d S T P . .
O1 O 0.40847(14) 0.30702(15) 0.20458(16) 0.0390(5) Uani 1 1 d . . . . .
C1 C 0.500000 0.2797(4) 0.2413(3) 0.0363(8) Uani 1 2 d S T P . .
H1 H 0.500000 0.233549 0.303211 0.044 Uiso 1 2 calc R U P . .
C2 C 0.500000 -0.0971(10) 0.000000 0.084(3) Uani 1 4 d DS TU P . .
H2A H 0.561(5) -0.153(5) 0.000000 0.101 Uiso 0.75 2 d DS U P . .
H2B H 0.500000 -0.1515(17) 0.0624(4) 0.101 Uiso 0.75 2 d DS U P . .
N1 N 0.437(3) 0.000000 0.000000 0.079(5) Uani 0.25 4 d DS TU P A 1
H3 H 0.395(6) 0.000000 0.062(4) 0.095 Uiso 0.25 2 d DS U P B 1
H4 H 0.442(4) 0.000000 -0.104(6) 0.095 Uiso 0.25 2 d DS U P C 2
N2 N 0.500000 -0.0262(13) -0.0643(15) 0.020(4) Uiso 0.125 2 d DS U P A 2
O2 O 0.552(3) 0.500000 0.500000 0.11(2) Uiso 0.1667 4 d DS . P . .
H5 H 0.602(6) 0.445(4) 0.500000 0.138 Uiso 0.1667 2 d DS U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3486 0.8531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 180.00(4) 45 9 ?
O1 Fe1 O1 91.42(7) 45 41 ?
O1 Fe1 O1 88.58(7) 9 41 ?
O1 Fe1 O1 88.58(7) 45 5 ?
O1 Fe1 O1 91.42(7) 9 5 ?
O1 Fe1 O1 180.00(9) 41 5 ?
O1 Fe1 O1 91.42(7) 45 37 ?
O1 Fe1 O1 88.58(7) 9 37 ?
O1 Fe1 O1 91.42(7) 41 37 ?
O1 Fe1 O1 88.58(8) 5 37 ?
O1 Fe1 O1 88.58(7) 45 . ?
O1 Fe1 O1 91.42(8) 9 . ?
O1 Fe1 O1 88.58(7) 41 . ?
O1 Fe1 O1 91.42(8) 5 . ?
O1 Fe1 O1 180.0 37 . ?
C1 O1 Fe1 129.2(2) . . ?
O1 C1 O1 126.8(3) . 28_655 ?
N2 C2 N2 84.3(19) 26 . ?
N1 C2 N1 66(2) 2_655 . ?
C2 N1 C2 114(2) . 25_655 ?
N2 N2 C2 137.8(10) 2_655 . ?
C2 N2 N2 47.8(10) . 26 ?
C2 N2 C2 110.3(15) . 25_655 ?
O2 O2 O2 60.002(8) 33_666 29_666 ?
O2 O2 O2 90.004(1) 33_666 9 ?
O2 O2 O2 60.002(3) 29_666 9 ?
O2 O2 O2 60.002(1) 33_666 5 ?
O2 O2 O2 90.0 29_666 5 ?
O2 O2 O2 60.002(1) 9 5 ?
O2 O2 O2 45.002(10) 33_666 25_666 ?
O2 O2 O2 45.002(11) 29_666 25_666 ?
O2 O2 O2 45.002(10) 9 25_666 ?
O2 O2 O2 45.002(7) 5 25_666 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.1014(17) 45 ?
Fe1 O1 2.1014(17) 9 ?
Fe1 O1 2.1014(17) 41 ?
Fe1 O1 2.1014(17) 5 ?
Fe1 O1 2.1014(17) 37 ?
Fe1 O1 2.1014(17) . ?
O1 C1 1.233(2) . ?
C2 N2 1.154(18) 26 ?
C2 N2 1.154(18) . ?
C2 N1 1.397(18) 2_655 ?
C2 N1 1.397(18) . ?
C2 N2 1.68(2) 2_655 ?
C2 N2 1.68(2) 4 ?
N2 N2 0.63(3) 2_655 ?
N2 N2 1.55(4) 26 ?
O2 O2 0.88(6) 33_666 ?
O2 O2 0.88(6) 29_666 ?
O2 O2 0.88(6) 9 ?
O2 O2 0.88(6) 5 ?
O2 O2 1.24(8) 25_666 ?
